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建立了离子液体均相液液微萃取-高效液相色谱法测定水中痕量双酚A的分析方法。通过一定浓度的加标回收率实验,优化了离子液体均相液液萃取的条件和高效液相色谱仪的条件。对影响萃取和样品制备条件的因素进行了优化,其中萃取条件包括离子液体种类、体积、NH4PF6的量、萃取时间和离心时间,而样品制备的条件包括pH和NaCl含量。优化的最佳条件是:90μL离子液体1-己基-3-甲基咪唑四氟硼酸盐离子液体([C_6MIM][BF_4])作萃取剂,NH_4PF_6和[C_6MIM][BF_4]的摩尔比为6:1,萃取1.0 min,离心8.0 min,调节样品溶液的pH为8.0,NaCl质量分数为6.0%。在此条件下,双酚A在1.25~100μg/L范围内线性良好,相关系数大于0.999,回收率为86.5%~118.8%,相对标准偏差为2.5%~8.5%,定量限为1.25μg/L。
An analytical method for the determination of trace amount of bisphenol A in water by ion-liquid homogeneous liquid-liquid microextraction and high performance liquid chromatography was established. Through a certain concentration of spiked recoveries experiments, the conditions of homogeneous liquid-liquid extraction of Ionic Liquids and the conditions of High Performance Liquid Chromatography were optimized. Factors affecting the extraction and sample preparation conditions were optimized, including the type of ionic liquid, the volume, the amount of NH4PF6, the extraction time and the centrifugation time, while the conditions for sample preparation included pH and NaCl. The optimum conditions for the optimization were: 90μL ionic liquid 1-hexyl-3-methylimidazolium tetrafluoroborate ionic liquid ([C_6MIM] [BF_4]) as extractant, the molar ratio of NH_4PF_6 and [C_6MIM] [BF_4] 6: 1, extracted for 1.0 min, centrifuged for 8.0 min, the pH of the sample solution was adjusted to 8.0, and the mass fraction of NaCl was 6.0%. Under this condition, the linear range of BPA was 1.25 ~ 100μg / L, the correlation coefficient was greater than 0.999, the recovery was 86.5% -118.8%, the relative standard deviation was 2.5% -8.5%, and the limit of quantification was 1.25μg / L .